CN106564873A - Novel macro- and micro-porous thin film carbon material and preparation method of same - Google Patents
Novel macro- and micro-porous thin film carbon material and preparation method of same Download PDFInfo
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- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
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Abstract
The invention discloses a novel macro- and micro-porous thin film carbon material and a preparation method of same. The method includes the steps of supporting polydopamine thin film on hollow spherical calcium carbonate as a template agent; performing high-temperature carbonization to obtain an inter-product CaO@S-HFGB; washing the CaO@S-HFGB in water to neutral and filtering the liquid to obtain a filter cake; and drying the filter cake to produce the novel macro- and micro-porous thin film carbon material. During the high-temperature carbonization, the hollow spherical calcium carbonate is decomposed and releases CO2, which has high effect on pore enlarging, so that secondary carbonization and requirement of introduction of a pore enlarging agent are avoided. The method can produce the porous carbon material S-HFGB just through one-step carbonization. The method is simple, is green, energy-saving and environment-friendly, and has great application potential in industrialization.
Description
Technical field
The invention belongs to material chemistry technical field, and in particular to a kind of new big micro-diplopore thin film material with carbon element and its preparation
Method.
Background technology
Porous carbon materials are cheap due to its as a kind of environmentally friendly material, high-specific surface area, pore structure can
The advantages of modified and excellent heat stability so as to have at aspects such as gas absorption, ultracapacitor, catalyst carriers
Very big application potential.And there are the porous carbon materials of special appearance structure, in application sides such as gas separation, medicament slow release, catalysis
The excellent properties that face shows so as to which correlation prepares the study hotspot for becoming scientists.
Hard template method is a kind of common method for being effectively synthesized porous carbon materials, typically has following step to constitute：(1)
Carbon matrix precursor is immersed in template；(2) allow presoma to be polymerized in template, specific morphology is obtained by high temperature cabonization
Material with carbon element；(3) template in material with carbon element is removed；(4) expanding agent is added in specific morphology material with carbon element, carries out high temperature cabonization expansion
Hole, is obtained the porous carbon materials with special appearance.Common spherical template agent has silicon dioxide, ferroso-ferric oxide etc., but deposits
The problems such as material with carbon element pattern after the difficult removal of template, removal easily caves in.Additionally, in traditional hard template method, needing
Through carburising step twice and add expanding agent, can be only achieved effect of material with carbon element reaming, had a strong impact on product yield and energy
Consumption.
Calcium Carbonate is a kind of common inorganic material, many advantages, such as with cheap, nontoxic, good biocompatibility.
The calcium carbonate product of different-shape can be prepared using processing method, the difference of crystallization condition, can be applied to as template many
In the preparation of hole material with carbon element.Dopamine (dopamine), is a kind of biological neural mediator, and under aqueous conditions, it can be molten
There is oxidation-cross-linking reaction in the presence of solution oxygen, form the compound thin layer of poly-dopamine that strength is attached to solid material surface
(PDA), can be used as the presoma of special appearance material with carbon element.
The disclosure of background above technology contents is only used for design and the technical scheme for aiding in understanding the present invention, and it is not necessarily
Belong to the prior art of present patent application, without tangible proof show the above present patent application the applying date
In the case of disclosed, above-mentioned background technology should not be taken to evaluate the novelty and creativeness of the application.
The content of the invention
The technical problem to be solved in the present invention is to provide a kind of new big micro-diplopore thin film material with carbon element and preparation method thereof, with
Solve the difficult removal of conventional template agent, the loaded down with trivial details problem of the reaming program that is carbonized.The present invention during high temperature cabonization, composite
CaCO3Calcium Carbonate in@PDA not only acts as pattern supporting role, the CO of its pyrolytic release2Also there is efficient reaming effect；
The inventive method, solve traditional spheroidal template it is difficult remove, pattern easily caves in problem, while avoiding secondary carbonization and needing
Introduce the problem of expanding agent.
In order to solve above technical problem, the present invention is employed the following technical solutions：
For this purpose, the present invention proposes a kind of new big micro-diplopore thin film material with carbon element, it is template using hollow sphere Calcium Carbonate,
Load poly-dopamine thin film, obtains intermediate product CaO@S-HFGB under high temperature cabonization, then washes CaO@S-HFGB with water extremely
Neutrality simultaneously filters to obtain filter cake, by filtration cakes torrefaction, new big micro-diplopore thin film material with carbon element is obtained.
The present invention also provides a kind of preparation method of new big micro-diplopore thin film material with carbon element, comprises the following steps：
(1) synthesis of hollow sphere Calcium Carbonate
Aqueous povidone solution 600mL, calcium chloride water 800mL, aqueous sodium carbonate 800mL are prepared respectively
With sodium dodecyl sulfate aqueous solution 600mL, four kinds of different solutions seal stir respectively；Take two parts of volumes and be 300mL
The polyvinylpyrrolidonesolution solution for preparing, is added in the calcium chloride solution and sodium carbonate liquor for preparing respectively simultaneously,
Under 20 DEG C of water bath conditions, 0.5h is stirred vigorously；Then the sodium dodecyl sulfate solution for preparing is added to into above-mentioned sodium carbonate
Solution, is stirred vigorously 0.5h；Above-mentioned calcium chloride solution is added in the mixed solution of sodium carbonate, in 20 DEG C of bath temperature, is stirred
Mix rotating speed 300rmin-1Under conditions of, react 2h；Reaction rear slurry is carried out into sucking filtration, is washed with dehydrated alcohol and deionization
Wash, the above is operated in triplicate, 80 DEG C of vacuum drying 5h are obtained hollow sphere Calcium Carbonate；
(2)CaCO3The preparation of@PDA composites
Dopamine saline solution 100mL, hollow sphere calcium carbonate aqueous solution 50mL are prepared respectively, and by 0.75mL ammonia
Water, 40mL ethanol, the alkaline solution that 90mL deionized waters are prepared, three kinds of different solutions seal stir respectively；To configure
Calcium carbonate aqueous solution add into DOPA amine salt aqueous solution, in 15～25 DEG C of bath temperature, 150～300r of speed of agitator
min-1Under conditions of, react 0.5h；The alkaline solution for preparing is added in above-mentioned dopamine mixed salt solution, reaction temperature
Keep constant with rotating speed, react 20h；Reaction rear slurry is carried out sucking filtration, is washed with deionized, 80 DEG C of vacuum drying 5h, system
Obtain CaCO3@PDA composites；
(3) preparation of new big micro-diplopore thin film material with carbon element
Weigh the CaCO of certain mass3@PDA composite samples are placed in tube furnace, under the protection of nitrogen, carry out height
Temperature carbonization, obtains intermediate product CaO@S-HFGB, and deionized water is washed to neutrality, finally filter cake is put into into 80 DEG C true
5h is dried in empty drying baker, new big micro-diplopore thin film material with carbon element is obtained.
Further, the concentration of aqueous povidone solution described in step (1) is 20gL-1。
Further, the concentration of calcium chloride water described in step (1) is 0.1molL-1。
Further, the concentration of aqueous sodium carbonate described in step (1) is 0.1molL-1。
Further, concentration 0.05molL of sodium dodecyl sulfate aqueous solution described in step (1)-1。
Further, the concentration of dopamine saline solution described in step (2) is 3～7gL-1。
Further, the concentration of hollow sphere calcium carbonate aqueous solution described in step (2) is 8gL-1。
Further, rear slurry washing is reacted described in step (2) and takes steps of processing, will reaction rear slurry with having
Machine filter film carries out sucking filtration, and deionized water is supplemented when filtrate is down to half in funnel to full bucket, and the above is operated in triplicate；Will filter
Cake is dissolved in deionized water, is slowly stirred 4h, and washing film with water carries out sucking filtration, is repeated twice by first time sucking filtration process, finally will
Filter cake is put in 80 DEG C of vacuum drying oven and is dried 5h.
Further, high temperature cabonization program is comprised the following steps described in step (3)：
(a) temperature-rise period：With 2～10 DEG C of min-1Speed by CaCO3@PDA composite samples rise to 700 from room temperature
～900 DEG C；
(b) thermostatic process：By CaCO3@PDA composite samples keep 1～3h at 700～900 DEG C；
(c) temperature-fall period：Presoma is naturally cooled to into room temperature from 700～900 DEG C.
The present invention compared with prior art, has the advantages that：
(1) present invention resolves into calcium oxide and carbon dioxide using hollow sphere Calcium Carbonate as template after high temperature cabonization,
Calcium oxide is can remove with water, is solved the problems, such as that later stage template is difficult and is removed；
(2) the hollow sphere Calcium Carbonate used by the present invention, during high temperature cabonization, it decomposes the CO of release2With height
Effect reaming effect, it is to avoid secondary carbonization and need to introduce the problem of expanding agent, one step carbonization can obtain porous carbon materials S-
HFGB；
(3) one step carbonization of the invention, sends out compared to traditional two steps carbonization, and product yield is higher；
(4) product of preparation of the invention, structure novel has big micro-diplopore structure, and specific surface area is higher；
(5) preparation method of the invention is simple, process energy-saving and environment friendly, has greatly application latent in industrialization
Energy.
Description of the drawings
Fig. 1 is the SEM and TEM figure of the hollow sphere Calcium Carbonate of the embodiment of the present invention one and S-HFGB；
Fig. 2 is S-HFGB constituent content analysis figures after the composite CaO@S-HFGB of the embodiment of the present invention one and washing；
Fig. 3 is the hollow sphere Calcium Carbonate of the embodiment of the present invention one, the XRD figure of CaO@S-HFGB and S-HFGB；
Fig. 4 is the hollow sphere Calcium Carbonate of the embodiment of the present invention one, CaCO3The TG figures of@PDA；
Fig. 5 is the N of the S-HFGB of the embodiment of the present invention one2Adsorption-desorption figure.
Specific embodiment
With reference to specific embodiment and compare accompanying drawing the present invention is described in further detail.It is emphasized that
What the description below was merely exemplary, rather than in order to limit the scope of the present invention and its application.
Embodiment 1
A kind of preparation method of new big micro-diplopore thin film material with carbon element, comprises the following steps：
(1) synthesis of hollow sphere Calcium Carbonate
Difference compound concentration 20gL-1Polyvinylpyrrolidone (PVP) aqueous solution 600mL, concentration 0.1molL-1's
Calcium chloride (CaCl2) aqueous solution 800mL, concentration 0.1molL-1Sodium carbonate (Na2CO3) aqueous solution 800mL and concentration
0.05mol·L-1Dodecyl sodium sulfate (SDS) aqueous solution 600mL, four kinds of different solutions seal stir respectively；Take two
The PVP solution that part (each 300mL) prepares, is added to the CaCl for preparing simultaneously respectively2Solution and Na2CO3In solution, 20
Under DEG C water bath condition, 0.5h is stirred vigorously；Then the SDS solution for preparing is added to into above-mentioned Na2CO3Solution, is stirred vigorously
0.5h；By above-mentioned CaCl2Solution adds Na2CO3Mixed solution in, in 20 DEG C of bath temperature, speed of agitator 300rmin-1
Under conditions of, react 2h；Will reaction rear slurry carry out sucking filtration, with dehydrated alcohol and deionized water wash, above operation repeats three
Secondary, 80 DEG C of vacuum drying 5h are obtained hollow sphere calcium carbonate product；
(2)CaCO3The preparation of@PDA composites
Compound concentration is 5gL-1DOPA amine salt (DA) aqueous solution 100mL, concentration 8gL-1Hollow sphere Calcium Carbonate is water-soluble
Liquid 50mL, i.e. part by weight are 1.25DA/1.0CaCO3DOPA amine salt and hollow sphere Calcium Carbonate, and by 0.75mL ammonia
Water, 40mL ethanol, the weakly alkaline solution that 90mL deionized waters are prepared, three kinds of different solutions seal stir respectively；Will configuration
Good calcium carbonate aqueous solution is added into DOPA amine salt aqueous solution, in 20 DEG C of bath temperature, speed of agitator 200rmin-1Bar
Under part, 0.5h is reacted；The weakly alkaline solution for preparing is added in above-mentioned dopamine mixed salt solution, reaction temperature and rotating speed
Keep constant, react 20h；Reaction rear slurry is carried out sucking filtration, is washed with deionized, 80 DEG C of vacuum drying 5h are obtained
CaCO3@PDA composites；
(3) preparation of new big micro-diplopore thin film material with carbon element
Weigh the CaCO of certain mass3@PDA samples are placed in tube furnace, under the protection of nitrogen, carry out high temperature cabonization,
Carbonization Conditions are：With 5 DEG C of min-1Speed by CaCO3@PDA samples rise to 700 DEG C from room temperature, constant temperature 1h, then natural cooling
To room temperature；Intermediate product CaO@S-HFGB are obtained, deionized water is washed to neutrality, it is final to obtain material with carbon element S-HFGB-
1。
Embodiment 2
Become outside the pale of civilization except following, remaining is with embodiment 1.
Compound concentration is 3gL-1DOPA amine salt (DA) aqueous solution 100mL, concentration 8gL-1Hollow sphere Calcium Carbonate is water-soluble
Liquid 50mL, i.e. part by weight are 0.75DA/1.0CaCO3DOPA amine salt and hollow sphere Calcium Carbonate, and by 0.75mL ammonia
Water, 40mL ethanol, the weakly alkaline solution that 90mL deionized waters are prepared, three kinds of different solutions seal stir respectively；Will configuration
Good calcium carbonate aqueous solution is added into DOPA amine salt aqueous solution, in 15 DEG C of bath temperature, speed of agitator 150rmin-1Bar
Under part, 0.5h is reacted；The weakly alkaline solution for preparing is added in above-mentioned dopamine mixed salt solution, reaction temperature and rotating speed
Keep constant, reaction 20h is obtained intermediate product CaCO3@PDA；
Weigh the CaCO of certain mass3@PDA samples are placed in tube furnace, under the protection of nitrogen, carry out high temperature cabonization,
Carbonization Conditions are：With 2 DEG C of min-1Speed by CaCO3@PDA samples rise to 800 DEG C from room temperature, constant temperature 2h, then natural cooling
To room temperature；Intermediate product CaO@S-HFGB are obtained, deionized water is washed to neutrality, it is final to obtain material with carbon element S-HFGB-
2。
Embodiment 3
Become outside the pale of civilization except following, remaining is with embodiment 1.
Compound concentration is 6gL-1DOPA amine salt (DA) aqueous solution 100mL, concentration 8gL-1Hollow sphere Calcium Carbonate is water-soluble
Liquid 50mL, i.e. part by weight are 1.5DA/1.0CaCO3DOPA amine salt and hollow sphere Calcium Carbonate, and by 0.75mL ammonia,
40mL ethanol, the weakly alkaline solution that 90mL deionized waters are prepared, three kinds of different solutions seal stir respectively；By what is configured
Calcium carbonate aqueous solution is added into DOPA amine salt aqueous solution, in 25 DEG C of bath temperature, speed of agitator 300rmin-1Under conditions of,
Reaction 0.5h；The weakly alkaline solution for preparing is added in above-mentioned dopamine mixed salt solution, reaction temperature keeps with rotating speed
Constant, reaction 20h is obtained intermediate product CaCO3@PDA；
Weigh the CaCO of certain mass3@PDA samples are placed in tube furnace, under the protection of nitrogen, carry out high temperature cabonization,
Carbonization Conditions are：With 10 DEG C of min-1Speed by CaCO3@PDA samples rise to 900 DEG C from room temperature, constant temperature 3h, then natural cooling
To room temperature；Intermediate product CaO@S-HFGB are obtained, deionized water is washed to neutrality, it is final to obtain material with carbon element S-HFGB-
3。
Instance analysis
As shown in figure 1, S-HFGB porous carbon materials prepared by the present invention, the appearance structure with hollow sphere shows mould
Plate agent Calcium Carbonate has resolved into completely calcium oxide and has been washed with water removal, and pattern caves in after wash water.The wherein bright grain of SEM charts
Footpath is about 5 μm of hollow sphere Calcium Carbonate, is mutually to be piled up to form by the platy particle of many uniform particle diameters, aligned orderly.
As shown in Fig. 2 S-HFGB its phosphorus content prepared by the present invention is up to 84.5%；After wherein CaO@S-HFGB and washing
Calcium element content in S-HFGB, respectively 15.3% and 0.26%, show that calcium oxide has been washed with water completely removal.
As shown in figure 3, hollow sphere Calcium Carbonate prepared by the present invention is calcite type, and intermediate product CaO@S-HFGB
XRD spectrum without the characteristic peak of Calcium Carbonate calcite type, shows CaCO3Calcium Carbonate in@PDA has resolved into completely calcium oxide.
Wherein the XRD figure of S-HFGB, has graphitization characteristic peak on 26 ° and 44 °, and (002) and (100) crystal face shows that S-HFGB has
There is part carbonization structure.
As shown in figure 4, the hollow sphere Calcium Carbonate and CaCO of present invention preparation3@PDA decomposition temperatures, respectively 605 DEG C and
675 DEG C, wherein CaCO3@PDA weight-loss ratios under conditions of greenhouse rises to 900 DEG C are about 55%.
As shown in figure 5, the N of the S-HFGB of present invention preparation2Adsorption/desorption figure, and its thus obtain the pore structure of material
As shown in table 1.Understand that S-HFGB has high-specific surface area and big micro-diplopore structure, BET and Langmuir specific surface areas are respectively
719.9m2·g-1, 955.6m2·g-1, wherein micropore ratio is 26.08%.
The pore structure parameter of the S-HFGB of table 1
It would be recognized by those skilled in the art that it is possible that numerous accommodations are made to above description, so embodiment and attached
Figure is intended merely to describe one or more particular implementations.
Although having been described above and describing the example embodiment for being counted as the present invention, it will be apparent to those skilled in the art that
It can be variously modified and be replaced, without departing from the spirit of the present invention.Furthermore it is possible to make many modifications with by spy
Condition of pledging love is fitted to the religious doctrine of the present invention, without departing from invention described herein central concept.So, the present invention is unrestricted
May also include belonging to all embodiments and its equivalent of the scope of the invention in specific embodiment disclosed here, but the present invention
Thing.
Claims (10)
1. a kind of new big micro-diplopore thin film material with carbon element, it is characterised in that：It is template using hollow sphere Calcium Carbonate, load is poly-
Dopamine thin film, obtains intermediate product CaO@S-HFGB under high temperature cabonization, then wash with water CaO@S-HFGB to it is neutral simultaneously
Filter cake is filtered to obtain, by filtration cakes torrefaction, new big micro-diplopore thin film material with carbon element is obtained.
2. a kind of preparation method of new big micro-diplopore thin film material with carbon element according to claim 1, it is characterised in that include
Following steps：
(1) synthesis of hollow sphere Calcium Carbonate
Aqueous povidone solution 600mL, calcium chloride water 800mL, aqueous sodium carbonate 800mL and ten are prepared respectively
Dialkyl sulfonates aqueous solution 600mL, four kinds of different solutions seal stir respectively；Take two parts of volumes and be 300mL preparations
Good polyvinylpyrrolidonesolution solution, is added in the calcium chloride solution and sodium carbonate liquor for preparing respectively, at 20 DEG C simultaneously
Under water bath condition, 0.5h is stirred vigorously；Then the sodium dodecyl sulfate solution for preparing is added to into above-mentioned sodium carbonate liquor,
It is stirred vigorously 0.5h；Above-mentioned calcium chloride solution is added in the mixed solution of sodium carbonate, in 20 DEG C of bath temperature, speed of agitator
300r·min-1Under conditions of, react 2h；Will reaction rear slurry carry out sucking filtration, with dehydrated alcohol and deionized water wash, the above
In triplicate, 80 DEG C of vacuum drying 5h are obtained hollow sphere Calcium Carbonate for operation；
(2)CaCO3The preparation of@PDA composites
Dopamine saline solution 100mL, hollow sphere calcium carbonate aqueous solution 50mL are prepared respectively, and by 0.75mL ammonia,
40mL ethanol, the alkaline solution that 90mL deionized waters are prepared, three kinds of different solutions seal stir respectively；By the carbon for having configured
Sour calcium aqueous solution is added into DOPA amine salt aqueous solution, in 15～25 DEG C of bath temperature, 150～300rmin of speed of agitator-1's
Under the conditions of, react 0.5h；The alkaline solution for preparing is added in above-mentioned dopamine mixed salt solution, reaction temperature and rotating speed
Keep constant, react 20h；Reaction rear slurry is carried out sucking filtration, is washed with deionized, 80 DEG C of vacuum drying 5h are obtained
CaCO3@PDA composites；
(3) preparation of new big micro-diplopore thin film material with carbon element
Weigh the CaCO of certain mass3@PDA composite samples are placed in tube furnace, under the protection of nitrogen, carry out pyrocarbon
Change, obtain intermediate product CaO@S-HFGB, deionized water is washed to neutrality, finally does the vacuum that filter cake is put into 80 DEG C
5h is dried in dry case, new big micro-diplopore thin film material with carbon element is obtained.
3. the preparation method of new big micro-diplopore thin film material with carbon element according to claim 2, it is characterised in that step (1)
Described in aqueous povidone solution concentration be 20gL-1。
4. the preparation method of new big micro-diplopore thin film material with carbon element according to claim 2, it is characterised in that step (1)
Described in calcium chloride water concentration be 0.1molL-1。
5. the preparation method of new big micro-diplopore thin film material with carbon element according to claim 2, it is characterised in that step (1)
Described in aqueous sodium carbonate concentration be 0.1molL-1。
6. the preparation method of new big micro-diplopore thin film material with carbon element according to claim 2, it is characterised in that step (1)
Described in sodium dodecyl sulfate aqueous solution concentration 0.05molL-1。
7. the preparation method of new big micro-diplopore thin film material with carbon element according to claim 2, it is characterised in that：Step (2)
Described in dopamine saline solution concentration be 3～7gL-1。
8. the preparation method of new big micro-diplopore thin film material with carbon element according to claim 2, it is characterised in that：Step (2)
Described in hollow sphere calcium carbonate aqueous solution concentration be 8gL-1。
9. the preparation method of new big micro-diplopore thin film material with carbon element according to claim 2, it is characterised in that：Step (2)
Described in react rear slurry washing take steps of processing, will reaction rear slurry carry out sucking filtration with organic filter membrane, when in funnel
Filtrate supplements deionized water to full bucket when being down to half, the above is operated in triplicate；Filter cake is dissolved in deionized water, is slowly stirred
4h is mixed, washing film with water carries out sucking filtration, be repeated twice by first time sucking filtration process, filter cake is finally put into 80 DEG C of vacuum drying oven
In be dried 5h.
10. the preparation method of new big micro-diplopore thin film material with carbon element according to claim 2, it is characterised in that：Step (3)
Described in high temperature cabonization program comprise the following steps：
(a) temperature-rise period：With 2～10 DEG C of min-1Speed by CaCO3@PDA composite samples rise to 700 from room temperature～
900℃；
(b) thermostatic process：By CaCO3@PDA composite samples keep 1～3h at 700～900 DEG C；
(c) temperature-fall period：By CaCO3@PDA composite samples naturally cool to room temperature from 700～900 DEG C.
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| CN109607510A (en) * | 2019-01-15 | 2019-04-12 | 广西大学 | ZIF base nitrogen-doped porous carbon material and preparation method thereof |
| CN109607510B (en) * | 2019-01-15 | 2022-04-05 | 广西大学 | ZIF-based nitrogen-doped porous carbon material and preparation method thereof |
| CN109864066A (en) * | 2019-03-22 | 2019-06-11 | 贺州学院 | Cypermethrin/chlopyrifos calcium carbonate controlled release agent and preparation method thereof |
| CN109938016A (en) * | 2019-03-22 | 2019-06-28 | 贺州学院 | Diacloden calcium carbonate sustained release agent and preparation method thereof |
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